CN109470767A - A kind of measuring method of Available Molybdenum in Soil - Google Patents
A kind of measuring method of Available Molybdenum in Soil Download PDFInfo
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Abstract
The invention discloses a kind of measuring methods of Available Molybdenum in Soil, by the way that digestion agent is added into soil, the effective molybdenum ion being swapped out in soil, the molybdenum ion of solution enters the atomization system of Inductively coupled plasma mass spectrometry in the form of an aerosol, object element goes out characteristic spectral line by gasification, ionization, exciting radiation in plasma flare, the concentration of effective molybdenum in solution is calculated according to Beer-Lambert Law, and then calculates the content of Available Molybdenum in Soil.This method does not specially require the property and composition of soil, and clay, sand, loam are suitable for this method.This method effectively extracts out the molybdenum element in soil using digestion agent, recycles Inductively coupled plasma mass spectrometry fast and accurately to determine the concentration of Molybdenum in Solution element, and then calculate the content of the Available Molybdenum in Soil.
Description
Technical field
The present invention relates to chemical substance analysis determining technology fields, and in particular to a kind of measurement side of Available Molybdenum in Soil
Method.
Background technique
Since the 1990s, great variety is had occurred in the research field of International Geological and scientific development direction,
Middle earth ecology investigation achieves the development advanced by leaps and bounds, and work basic for this, public welfare only measures element total amount
It is the demand for development for not being able to satisfy modern society.Therefore ecologic biological activity, the member of the morphological analysis especially element of element
The migration and biological effectiveness of element, chemically and physically behavior is essential to element morphology, it is necessary to illustrate beneficial element
Validity, the toxicity of harmful element, and the influence to environment.Contemporary science man has accepted a fact, element it is total
Concentration is not sufficient to evaluate its toxicity, helpfulness and biological effectiveness, can even misunderstand sometimes, it is believed that element total amount
Content is higher, and the biological effectiveness of element is higher.Molybdenum content in soil is generally very low, and effective molybdenum is molybdenum element in soil
A kind of existing forms, play an important role in growing process, especially the demand of pulse family and Cruciferae to molybdenum
It is very big, it mainly include water-soluble molybdenum, exchangeability molybdenum, slightly solubility molybdenum, organically combine state molybdenum etc..The content of Available Mo In Soil is to determine
Molydbenum fertilizer has unfruitful principal element, so effectively Molybdenum determination has great directive significance for agricultural production.
Mainly there are citric acid extraction, oxalic acid-ammonium oxalate to soak the leach extraction method of Available Molybdenum in Soil in the world at present
Formulation, ultrasound-assisted extraction method etc..Wherein effective molybdenum of citric acid extraction measurement absorbs correlation r=between molybdenum with vegetables
0.851 (n=22) has fairly good correlation, but since extraction efficiency is low, the result precision of measurement is poor.Oxalic acid-grass
Sour ammonium extraction mainly extracts water-soluble state molybdenum and exchange state molybdenum in soil, has preferable extraction effect；Ultrasound-assisted extraction
Method accelerates the leaching of ingredient to be measured to extract using the cavitation of ultrasonic wave, and the second order effect of ultrasonic wave can speed up extract component
Dispersal events, accelerate leaching rate.
Mainly have for the main measuring methods of leaching liquor；Colorimetric method, Catalytic Polarography, atomic absorption spectrography (AAS).Sulphur cyanogen
Hydrochlorate colorimetric method detection limit is higher, is unsuitable for the analysis of low content sample, and sample needs to extract, separation, enrichment, and operation is multiple
It is miscellaneous, need the time longer；Catalytic Polarography is higher for ambient temperature requirements, and the dropping-mercury electrode environmental pollution of application is very big,
This method is seldom applied at present；When atomic absorption spectrography (AAS) is using acetylene-air flame measurement sample, molybdenum element atom
It is very low to change efficiency, therefore it is lower to measure molybdenum element sensitivity, and by alkaline-earth metal serious interference in continuous mode.
In conclusion the measuring method of Available Molybdenum in Soil has certain requirement to the content of the molybdenum in soil at present, also
There is no the detection method of complete set that can be suitble to the detection of most Available Molybdenum in Soil.Therefore, a kind of be suitble to absolutely greatly is studied
The measuring method of the Available Molybdenum in Soil of part soil property has become urgent problem to be solved.
Summary of the invention
The technical problem to be solved by the present invention is in view of the shortcomings of the prior art, provide one kind to be suitble to various different soil
Effective molybdenum of earth property detect and for the content requirement of molybdenum relatively loose, experimental implementation process simple and flexible, it is at low cost, be convenient for
The measuring method for the Available Molybdenum in Soil that China promotes and applies.
In order to solve the above technical problems, the present invention adopts the following technical scheme: a kind of measuring method of Available Molybdenum in Soil,
It is characterized by: sample is measured in soil through oxalic acid-ammonium oxalate extraction (1:10) using icp ms
Effective molybdenum；
Sample enters radio frequency plasma by sampling system, and evaporation, dissociation, atomization and electricity in high temperature quarter bend
From ion is successively separated by bipyramid interface, ion mirror, level four bars mass analyzer, according to the size of mass/charge, finally
It is detected by ion detector, and with the amount of calibration curve quantitative analysis molybdenum, instrument response caused by sample matrices inhibits
Or enhancement effect and instrumental shift are compensated using internal standard；Specific determination step is as follows,
1) prepare reagent:
Oxalic acid-ammonium oxalate digestion agent, weighs 24.9g ammonium oxalate, and chemical formula is (NH4)2C2O4·H2O, excellent pure grade and 12.6g
Oxalic acid, chemical formula H2C2O4·2H2O, excellent pure grade are dissolved in water together, are settled to 1L, PH 3.3；
Hydrochloric acid, concentration 1+1, excellent pure grade；
2) molybdenum Standard Stock solutions, concentration are ρ (Mo)=1.00mg/mL；
Molybdenum standard solution, concentration are ρ (Mo)=1.00 μ g/mL: the preparation of molybdenum Standard Stock solutions is diluted with water, equivalent is added
Digestion agent medium；
3) prepare sample: being collected pedotheque, and remove the foreign matter in sample, including branch stick, blade, stone；
4) sample measures:
A, the air-dried pedotheque of 5.0g is weighed in plastics extraction flask, and 50mL oxalic acid-ammonium oxalate digestion agent is added, is stoppered
Bottle cap shakes up, and is placed on vibrating machine in 25 DEG C and vibrates 8h；It is dry with the processed middling speed quantitative filter paper of the HCl for being 1+1 through over-richness
Filtering divides and takes 30.0mL supernatant liquor, is placed on electric hot plate and is evaporated；450 DEG C of calcinations destroy oxalic acid and organic matter in high temperature furnace,
It takes out, it is cooling；Add the HCl that 1mL concentration is 1+1 to dissolve, be diluted with water to 10mL, is surveyed with inductively coupled plasma transmitting mass spectrography
It is fixed；
B, blank assay carries out while sample treatment, and in addition to sample is not added, other steps are carried out by a；
5) draw standard curve: draw respectively molybdenum standard solution 0.00,0.50,1.00,2.00,3.00,4.00mL in
In the volumetric flask of 100mL, with water constant volume, as 0.000,0.005,0.010,0.020,0.030, the 0.040 μ g/mL standard containing molybdenum
Serial solution；
By the instrument reference conditions of optimization, standard series is successively imported into atomizer from low concentration to high concentration and is divided
Analysis, using the mass concentration of object element as abscissa, corresponding emissive porwer value is ordinate, establishes standard curve, standard
The concentration range of curve is adjusted according to the concentration levels of element to be measured in actual sample；
6) calculated result
The content ω (mg/kg) of effective molybdenum in pedotheque is calculated according to the following formula:
In formula:
ω --- the content of effective molybdenum, unit mg/kg in pedotheque；
ρ --- the mass concentration of effective molybdenum in measurement sample, unit mg/L are checked in by standard curve；
ρ0--- the mass concentration of effective molybdenum, unit mg/L in the blank sample of laboratory；
The volume of leaching liquor, unit ml are added when prepared by V --- sample；
M --- weigh the quality of sample after sieving, unit g；
The extension rate of f --- sample；
Wdm--- pedotheque dry matter content, %.
In step 1), molybdenum Standard Stock solutions are prepared as follows: weighing light of the 0.7502g through 500 DEG C of calcination 1h
Spectrum pure zirconia molybdenum is placed in a beaker, and after the NaOH dissolution of 20mL 0.4g/L, is moved into 500mL volumetric flask, is 2+98 with concentration
H2SO4It is diluted to scale.
The nylon mesh that the sample of acquisition is air-dried in laboratory, roughly grinds, was finely ground to 10 mesh of aperture.
Used inductive coupling plasma emission spectrograph is instrument quality scanning range 5u~250u, minimum is differentiated
Rate be at 5% peak height 1u peak width, peristaltic pump threeway sample introduction, quadrupole rod Inductively coupled plasma mass spectrometry, RF power is
1.3kw, secondary air speed are 0.8L/min, cooling air flow velocity is 14L/min, atomization gas flow velocity is 1.0L/min, sampling taper hole
Diameter is 1.2mm, and interception taper hole diameter is 1.0mm；The argon gas used is high-purity grade, argon mass fraction >=99.99%.
The temperature control of constant temperature oscillator used is 25 ± 2 DEG C, oscillation frequency control is 160r/min~200r/min.
This method detection is limited to 0.02mg/kg.
The present invention is by the way that digestion agent is added into soil, the effective molybdenum ion being swapped out in soil, the molybdenum ion of solution with
The form of aerosol enters the atomization system of Inductively coupled plasma mass spectrometry, and object element is in plasma flare by gas
Change, ionization, exciting radiation go out characteristic spectral line, the concentration of effective molybdenum in solution are calculated according to Beer-Lambert Law, and then calculate
The content of Available Molybdenum in Soil out.This method does not specially require the property and composition of soil, and clay, sand, loam are suitable
For this method.This method effectively extracts out the molybdenum element in soil using digestion agent, utilizes inductive coupling plasma mass spectrometry
The powerful analysis power of test of instrument fast and accurately determines the concentration of Molybdenum in Solution element, and then calculates in the soil effectively
The content of molybdenum, fast, at low cost, high-efficient, technical process simple and flexible, low power consumption and other advantages, application prospect with analysis speed
It is very wide.
Specific embodiment
It is described further With reference to embodiment:
In the present embodiment, whole measurement process is sequentially included the following steps:
1, prepare reagent and material:
1.1 oxalic acid-ammonium oxalate digestion agent: 24.9g ammonium oxalate [(NH is weighed4)2C2O4·H2O, excellent pure grade] and 12.6g oxalic acid
(H2C2O4·2H2O, excellent pure grade) it is dissolved in water, it is settled to 1L.PH is 3.3；
1.2 molybdenum Standard Stock solutions ρ (Mo)=1.00mg/mL: spectrum pure oxygen of the 0.7502g through 500 DEG C of calcination 1h is weighed
Change molybdenum (MoO3) be placed in a beaker, after being dissolved with 20mL0.4g/LNaOH, move into 500mL volumetric flask, with (2+98) H2SO4It is dilute
It releases to scale；
1.3 molybdenum standard solution ρ (Mo)=1.00 μ g/mL: being diluted with water the preparation of molybdenum Standard Stock solutions, and equivalent extraction is added
Agent medium；
1.4 hydrochloric acid, concentration 1+1, excellent pure grade.
2, key instrument equipment:
2.1 nylon mesh: aperture 2.0mm (10 mesh)；
2.2 assay balances: sensibility reciprocal 0.1mg；
2.3 plastics extraction flasks；
2.4 controllable temperature oscillators, 25 DEG C ± 2 DEG C of temperature, frequency can be controlled in 160r/min~200r/min；
2.4 inductive coupling plasma emission spectrographs:
(a) instrument quality scanning range 5u~250u, minimum resolution are 1u peak width, peristaltic pump threeway at 5% peak height
Sample introduction, the running parameter by taking quadrupole rod Inductively coupled plasma mass spectrometry as an example are shown in Table 1；
(b) argon gas: high-purity grade (argon mass fraction >=99.99%).
3, sample acquisition and preparation:
3.1 sample collection and keeping
Relevant regulations acquisition and preservation pedotheque according to HJ/T 166.Sample acquisition, transport and preservation process should be kept away
Exempt to stain and element loss to be measured.
The measurement of 3.2 dry matter contents
The measurement of pedotheque dry matter content is executed according to HJ613.
3.3 sample preparation
The foreign matters such as branch stick, blade, the stone in sample are removed, according to the requirement of HJ/T 166, by the sample of acquisition in reality
Room is tested to be air-dried, roughly ground, being finely ground to aperture 2.0mm (10 mesh) nylon mesh.The preparation process of sample should be avoided contamination and to
Survey element loss.
4, determination step is analyzed:
4.1 sample pretreating
It weighs 5.0g (being accurate to 0.01g) and air-dries soil sample in plastics extraction flask, 50mL oxalic acid-ammonium oxalate extraction is added
Agent is stoppered bottle cap, shakes up, and is placed on vibrating machine in 25 DEG C and vibrates 8h.It is dry with the middling speed quantitative filter paper by (1+1) HCl processing
Filtering divides and takes 30.0mL supernatant liquor, is placed on electric hot plate and is evaporated, and 450 DEG C of calcinations destroy oxalic acid and organic matter in high temperature furnace.
It takes out, it is cooling, add 1mL (1+1) HCl to dissolve, be diluted with water to 10mL, emits mass spectrometric determination with inductively coupled plasma；
4.2 blank assay
Blank assay carries out while sample treatment, and in addition to sample is not added, other steps are by 4.1 operations.
The drafting of 4.3 standard curves
Respectively draw molybdenum standard solution (5.3) ρ (Mo)=1.00 μ g/mL (0.00,0.50,1.00,2.00,3.00,
4.00) mL is in 100mL volumetric flask, with water constant volume.As containing molybdenum (Mo) (0.000,0.005,0.010,0.020,0.030,
0.040) μ g/mL standard serial solution.
By the instrument reference conditions of optimization, standard series is successively imported into atomizer from low concentration to high concentration and is divided
Analysis.Using the mass concentration of object element as abscissa, corresponding emissive porwer value is ordinate, establishes standard curve, standard
The concentration range of curve can be adjusted according to the concentration levels of element to be measured in actual sample.
5, result calculates
The content ω (mg/kg) of effective molybdenum in pedotheque is calculated according to the following formula:
In formula:
ω --- the content of effective molybdenum, unit mg/kg in pedotheque；
ρ --- the mass concentration of effective molybdenum in measurement sample, unit mg/L are checked in by standard curve；
ρ0--- the mass concentration of effective molybdenum, unit mg/L in the blank sample of laboratory；
The volume of leaching liquor, unit ml are added when prepared by V --- sample；
M --- weigh the quality of sample after sieving, unit g；
The extension rate of f --- sample；
Wdm--- pedotheque dry matter content, %.
6, precision and accuracy
According to GB/T6392.2-2004, select standard substance 5 of different quality containing range, by 5 laboratories according to
This method carries out method precision experiment.Each horizontal sample is tested in each laboratory 5 times, and initial data is carried out statistical
Analysis.
Measurement result at most retains three effective digitals, unit mg/kg.
7, quality controls
The each analysis batch of sample should all be inserted into standard substance, repeat sample, while carry out blank assay.
7.1 every batch of samples at least make two laboratory blank samples, and measurement result should all be lower than Determination Limit；
7.2 each analyses should establish standard curve, and related coefficient answers >=0.999；
7.3 use arbitrary sampling method replicate analysis quantity for the 20%-30% of every Lot sample number；Sample number is no more than 5
When a, replicate analysis number is 100%；The quantity that special sample or the higher sample of quality requirement can take the circumstances into consideration to increase extraction sample is straight
To 100% analysis.
When 7.4 every analysis batch sample numbers are 10 or less, 1-2 standard substance control should be inserted into；At 10 or more, insert
Enter 2-3 standard substance monitoring；Special sample or the higher sample of quality requirement can take the circumstances into consideration to increase the monitoring quantity of standard substance.
7.5 other Con trolling index are executed by DZ/T0130.3.
In addition, when the molybdenum that is extracted of oxalic acid-ammonium oxalate digestion agent is below 0.15-2.0 μ g/mL, on acid soil
Leguminous plant has certain reaction to molydbenum fertilizer, and also needs further to verify to other plant.In addition to floristics, soil
Acidity also has an impact, and under different soils acidity, molybdenum gives property difference.The molybdenum that plant is absorbed, it is fast with increasing for P in soil H
Speed increase, have research and propose available " molybdenum value " evaluation soil in molybdenum supply values [molybdenum value=pH value+effectively molybdenum content (mg/kg ×
10)].When molybdenum value < 6.2, indicate that molybdenum supply is insufficient；When molybdenum value 6.2-8.2, indicate that molybdenum supply is medium；When molybdenum value > 8.2, molybdenum is indicated
Supply is sufficient.
Running parameter of the table 1 by taking certain quadrupole rod icp ms as an example
| Parameter | Setting value | Parameter | Setting value |
| ICP power | 1300w | Jump peak | 3 points/quality |
| Cooling gas flow | 14.0L/min | Residence time | 10ms/ point |
| Secondary air amount | 0.8L/min | Scanning times | 40 times |
| Atomization gas flow | 1.0L/min | Time of measuring | 60s |
| Sampling spiroid aperture | 1.2mm | Intercept taper hole diameter | 1.0mm |
The above has been described in detail, described above, is only a preferred embodiment of the present invention, when cannot
Limit practical range of the invention, i.e., it is all according to the made equivalent changes and modifications of the application range, it should still belong to the present invention and cover model
In enclosing.
Claims (5)
1. a kind of measuring method of Available Molybdenum in Soil, it is characterised in that: sample is extracted through oxalic acid-ammonium oxalate, using inductance coupling
Close effective molybdenum in plasma mass spectrograph measurement soil；
Sample enters radio frequency plasma by sampling system, and evaporation, dissociation, atomization and ionization in high temperature quarter bend, from
Son is successively separated by bipyramid interface, ion mirror, level four bars mass analyzer, according to the size of mass/charge, finally by ion
Detector is detected, and with the amount of calibration curve quantitative analysis molybdenum, and instrument response caused by sample matrices inhibits or enhancing
Effect and instrumental shift are compensated using internal standard；Specific determination step is as follows,
1) prepare reagent:
Oxalic acid-ammonium oxalate digestion agent, weighs 24.9g ammonium oxalate, and chemical formula is (NH4)2C2O4·H2O, excellent pure grade and 12.6g grass
Acid, chemical formula H2C2O4·2H2O, excellent pure grade are dissolved in water together, are settled to 1L, PH 3.3；
Hydrochloric acid, concentration 1+1, excellent pure grade；
2) molybdenum Standard Stock solutions, concentration are ρ (Mo)=1.00mg/mL；
Molybdenum standard solution, concentration are ρ (Mo)=1.00 μ g/mL: the preparation of molybdenum Standard Stock solutions is diluted with water, equivalent extraction is added
Agent medium；
3) prepare sample: being collected pedotheque, and remove the foreign matter in sample, including branch stick, blade, stone；
4) sample measures:
A, the air-dried pedotheque of 5.0g is weighed in plastics extraction flask, and 50mL oxalic acid-ammonium oxalate digestion agent is added, is stoppered bottle
Lid, shakes up, is placed on vibrating machine in 25 DEG C and vibrates 8h；It was done with the processed middling speed quantitative filter paper of the HCl for being 1+1 through over-richness
Filter divides and takes 30.0mL supernatant liquor, is placed on electric hot plate and is evaporated；450 DEG C of calcinations destroy oxalic acid and organic matter in high temperature furnace, take
Out, cooling；Add the HCl that 1mL concentration is 1+1 to dissolve, be diluted with water to 10mL, is surveyed with inductively coupled plasma transmitting mass spectrography
It is fixed；
B, blank assay carries out while sample treatment, and in addition to sample is not added, other steps are carried out by a；
5) it draws standard curve: drawing molybdenum standard solution 0.00,0.50,1.00,2.00,3.00,4.00mL respectively in 100mL's
In volumetric flask, with water constant volume, as 0.000,0.005,0.010,0.020,0.030, the 0.040 μ g/mL standard series containing molybdenum is molten
Liquid；
By the instrument reference conditions of optimization, standard series is successively imported into atomizer from low concentration to high concentration and is analyzed, with
The mass concentration of object element is abscissa, and corresponding emissive porwer value is ordinate, establishes standard curve, standard curve
Concentration range is adjusted according to the concentration levels of element to be measured in actual sample；
6) calculated result
The content ω (mg/kg) of effective molybdenum in pedotheque is calculated according to the following formula:
In formula:
ω --- the content of effective molybdenum, unit mg/kg in pedotheque；
ρ --- the mass concentration of effective molybdenum in measurement sample, unit mg/L are checked in by standard curve；
ρ0--- the mass concentration of effective molybdenum, unit mg/L in the blank sample of laboratory；
The volume of leaching liquor, unit ml are added when prepared by V --- sample；
M --- weigh the quality of sample after sieving, unit g；
The extension rate of f --- sample；
Wdm--- pedotheque dry matter content, %.
2. the measuring method of Available Molybdenum in Soil according to claim 1, it is characterised in that: in step 1), molybdenum standard
Stock solution is prepared as follows: weighing 0.7502g and is placed in a beaker through the spectroscopic pure molybdenum oxide of 500 DEG C of calcination 1h, uses
After the NaOH dissolution of 20mL 0.4g/L, moves into 500mL volumetric flask, be the H of 2+98 with concentration2SO4It is diluted to scale.
3. the measuring method of Available Molybdenum in Soil according to claim 1, it is characterised in that: testing the sample of acquisition
Room is air-dried, is roughly ground, was finely ground to the nylon mesh of 10 mesh of aperture.
4. the measuring method of Available Molybdenum in Soil according to claim 1, it is characterised in that: used inductive coupling etc.
Ionomer emission spectrum instrument is instrument quality scanning range 5u~250u, minimum resolution is 1u peak width, wriggling at 5% peak height
Pump threeway sample introduction, quadrupole rod Inductively coupled plasma mass spectrometry, RF power is 1.3kw, secondary air speed be 0.8L/min,
Cooling air flow velocity is 14L/min, atomization gas flow velocity is 1.0L/min, sampling spiroid aperture is 1.2mm, and interception taper hole diameter is 1.0mm；
The argon gas used is high-purity grade, argon mass fraction >=99.99%.
5. the measuring method of Available Molybdenum in Soil according to claim 1, it is characterised in that: constant temperature oscillator used
Temperature control is 25 ± 2 DEG C, oscillation frequency control is 160r/min~200r/min.
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| CN112326569A (en) * | 2020-10-21 | 2021-02-05 | 内蒙古国城实业有限公司 | Method for rapidly detecting molybdenum oxide minerals in molybdenum ore |
| CN112763571A (en) * | 2020-12-27 | 2021-05-07 | 江苏华测品标检测认证技术有限公司 | Method for testing effective molybdenum in soil |
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Application publication date: 20190315 |